Mission of the NMR Facility
The NMR facility is a service and research laboratory operated by and for the Department of Chemistry at Indiana University, Bloomington. The laboratory performs and assists in magnetic resonance spectroscopy activities that further the research goals of departmental faculty, post-doctoral fellows, students, and staff. The facility is available 24 hours per day for use by trained researchers. The following report summarizes the service and research activities of the NMR Facility during 1998.

Summary of Facilities
The NMR Facility includes the following Varian NMR spectrometers:

• Unity^Inova spectrometer operating at a 500 MHz ¹H Larmor frequency (I500)
• Unity^Inova spectrometer operating at a 400 MHz ¹H Larmor frequency (I400)
• VXR-Unity spectrometer operating at a 400 MHz ¹H Larmor frequency (VXR400)
• Gemini-2000 spectrometer operating at a 400 MHz ¹H Larmor frequency (Gem300)

In conjunction, four Sun workstations, one SGI workstation, and one Windows NT workstation provide processing, simulation, and administrative capabilities. A variety of probes are available for the observation of all possible nuclei and multinuclear experiments.

Summary of Research Activities
Research collaborations
Non-routine research collaborations include development of new NMR techniques and interpretation of spectra beyond daily interactions between Staff and Users. Research collaborations in 1998 include:

• two-dimensional experiments for the determination of biochemical structures (Novotny group)
• highly resolved two-dimensional experiments for analyses of polymer compositions (Chisholm group)
• surface water studies of salts (Ewing group)
• experiments observing ¹¹B (Todd group), ¹⁷O (Caulton group), ³⁵Cl (Prange Group, Medical Sciences), ⁵⁹Co (Christou group), and ²⁰⁷Pb (Caulton group)
• studies of chemical exchange reactions (Caulton & Chisholm groups)
• ³⁵Cl-hemoglobin binding studies (Prange Group, Medical Sciences)

Publications
Mubarak, M.S., Pagel, M., Marcus, L.M., & Peters, D.G. Formation of 2-(3'-Oxocyclohexyl)-2-cyclohexen-1-one via Reduction of 2-Cyclohexen-1-one with Electrogenerated Nickel (I) Salen. J. Org. Chem., vol. 63, pp. 1319-1322 (1998).

Baker, A., Zidek, L., Wiesler, D., Chmelik, J., Pagel, M., & Novotny, M.V. Reaction of N-Acetyl-Glycyl-Lysyl-Methyl Ester with 2-Alkenals: An Alternative Model for Covalent Modification of Proteins. Chem. Res. In Toxicol., vol. 11, pp. 730-740 (1998).

Chisholm, M.H., Iyer, S.S., McCollum, D.G., Pagel, M., & Werner-Zwanziger, U. Concerning the Microstructure of Poly(lactide, PLA, Phase-sensitive HETCOR Spectra of Poly(meso-lactide), Poly(recemic-lactide) and Atactic Poly(lactide). Macromolecules, in press.

Chen, P., Werner-Zwanziger, U., Weisler, D., Pagel, M., & Novotny, M.V., Mass Spectroscopic Analysis of Benzoylated Sialo-oligosaccharides and Differentiation of Terminal α2→3 and α2→6 Sialo-galactosidal Linkages at Subpicomole Levels. Anal. Chem., submitted for publication.

Chisholm, M.H., Crandall, J.K., McCollum, D.G., & Pagel, M. Concerning the Mechanism of Ring-Opening polymerization by Coordinate Catalysts: The 2D Homonuclear J-Resolved Spectrum of Poly(cyclohexene oxide). Submitted for publication.

Hollingsworth, M.D., Brown, M.E., Werner-Zwanziger, U., Hillier, A.C., Chaney, J.D., Still, E.J., & Vanecko, J.A., Superstructure Control of Shape and Ferroelasticity of Urea Inclusion Compounds in Self-Assembly in Synthetic Chemistry, Wuest, J.D., ed., NATO ASI Ser., Kluwer Academic Publishers, Dordrecht, The Netherlands, submitted for publication.

Poster Presentations
Guest Motions in Dihalohexane/Urea Inclusion Compounds studied by ¹H NMR, Werner-Zwanziger, U., Brown, M.E., Chaney, J.D., Still, E.J., & Hollingsworth, M.D., 29^th AMPERE-13 International Conference on Magnetic Resonance and Related Phenomena, Berlin, Germany, 8/2-7/98.

Guest Motions in Dihalohexane/Urea Inclusion Compounds studied by ¹H NMR, Werner-Zwanziger, U., Brown, M.E., Chaney, J.D., Still, E.J., & Hollingsworth, M.D., 39^th Experimental Nuclear Magnetic Resonance Conference, Pacific Grove, CA, 3/22-27/98.

Indiana Dynamics Database: WWW-Accessible Database of NMR Relaxation and Dynamics Parameters, Pagel, M.D., Goodman, J.L., & Stone, M.J., 39^th Experimental Nuclear Magnetic Resonance Conference, Pacific Grove, CA, 3/22-27/98.

Invited Seminars
Struktur and Dynamik von Gästen und Wirten in Dihalogenhexan/Harinstoff Einschluβverbindungen, Max-Planck-Institut für Medizinische Forschung, Heidelberg Germany, 6/10/98.

Structure and Dynamics of Hosts and Guests in Inclusion Compounds, Workshop of the Max-Planck-Institut für Polymerforschung, Schloβ Ringberg, Tegernsee, Germany, 4/22/98.

Honors
U. Werner Zwanziger, Professional Development Grant, Indiana University Bloomington Professional Council, 1998

U. Werner-Zwanziger, Visiting Scientist at the the Max-Planck-Institut für Polymerforschung, Mainz, Germany, 5/98 - 7/98.

Summary of Facility Services
Profile of Spectrometer Utilization
The NMR Facility is available 24 hours per day, each day of the year, for collaborative or independent use by trained researchers. The Graph Gallery shows the utilization of each spectrometer from Jan. 1 to Dec. 31, 1998, in several formats. The following observations (shown in bold) and interpretations are derived from the Graph Gallery:

• Utilization of the I500 is extremely high. The I500 is efficiently used by the biochemists at all times.
• The Gem300, VXR400, and datastations are most often used when researchers are in the building. These spectrometers and datastations used for short-term tasks requiring substantial user interaction (e.g., 1D experiments, data processing).
• The I400 is used more often when researchers are in the building, but overnight use is high (relative to the Gem300 and VXR400). The NMR Facility Staff most often uses/attends to the I400 (relative to other spectrometers). The I400 is used for both short-term and long-term tasks. The Staff uses the I400 to develop and perform long-term experiments in collaboration with researchers. The Staff also attends to regular I400 maintenance and development due probe changes, hardware modification & recabling, and user interaction to support an extremely large variety of experiments with this spectrometer.
• Overnight utilization of the I400, VXR400, and Gem300 is ~16%. Long-term experiment utilization is comparable to the estimate for this type of utilization (14%) used to determine the lower rate for long-term experiments
• Inorganic chemists dominate utilization of the Gem300 and I400. Organic chemists dominate the use of the VXR400. Biochemists are the primary users of the I500. The researchers of all research directions used all of the Datastations. The use of each spectrometer matches the NMR Facility utilization plan. Making the VXR400 available to inorganic chemists has not impacted the VXR400's availability for organic chemists. Similarly, permitting organic chemists to use the I400 has not impacted the I400's availability for inorganic chemists.

Notable services

• A new record of 76 consecutive days without breaking a sample in the NMR Facility was established, which is the result of an informal program to increase safety awareness. The previous record was 50 consecutive days.
• The Staff presented two lectures in C502 (Inorganic Spectroscopy) covering the basic procedures for one-dimensional and two-dimensional NMR experiments.
• The Associate Instructors of C344 used the VXR400 spectrometer for class work, with almost no impact on researchers.
• The Staff collected spectra of 23 samples prepared by the senior-level organic chemistry class of the Department of Chemistry at IPFW; this work assisted IPFW during a failure of their spectrometer facilities.
• The Staff consulted with Dr. Maggie Hupcey of the Sabin Corp., Bloomington, IN concerning the NMR spectroscopy of polymers.
• The Staff assisted in the acquisition of a donated 200 MHz NMR instrument for the teaching laboratory, which will arrive in Spring 1999. The Staff also conducted a site preparation survey for the new instrument.

Summary of Facility Developments
Spectrometer Improvements

• A second waveform generator board for the I500 spectrometer was installed for multidimensional experiments.
• Hardware and experimental procedures were extensively modified for faster and more reliable low-temperature experiments.
• A "broadband probe" day was initiated for setup of the I400 for less commonly used nuclei to meet needs of users while keeping wear of probes to a minimum.
• All workstations (except the I500) were upgraded to VNMR v6.1, which provides new opportunities for new experiments and other software developments. The VXR400 and NMRSUN1 workstations were upgraded to the Solaris 2.5 operating system to improve operating performance. The VXR400 workstation was upgraded from a Sparc2 to a Sparc5 model to improve operating speed.

Experiment Improvements

• Phase-sensitive versions of many experiments were implemented to improve spectral resolution.
• 14 MAGICAL II™ macros were developed for Varian-based NMR experiments and data processing.

Laboratory Improvements

• The frequency synthesizer was modified by the NMR Facility Staff to include frequency markers.
• The MAGnet REServation scheduling system was implemented for I400 scheduling in Feb. 1998, and implemented for scheduling other spectrometers in June 1998. This system allows users to reserve spectrometer time via web browsers, and replaced the paper-based system. A demo version of the MAG RES system and a freeware version were also made available via the NMR Facility web site.
• A HP4MV printer was installed, providing both 8x11 and 11x17 paper sizes. Color printing was also implemented. A software methodology for automatically selecting printing characteristics was developed by Dr. Marty Berliner. With Dr. Berliner's assistance, printing was also reconfigured so that the print request is routed directly to networked printers, which improved printing reliability.
• The NMRSUN2 workstation was upgraded from a Sparc5 to an UltraSparc5 model to meet the increasing demands for processing large data sets. A Sparc2 workstation (formerly on the VXR400 spectrometer) was converted to a data processing/administration station, relieving the NMRSUN3 workstation of administration duties.
• A routine, user-accessible backup system using CDROM and Zip disks was developed.
• Software for predicting ¹H and ¹³C chemical shifts, and software for spectral simulations based on chemical structures, was installed on the laboratory PC workstation.
• The I400 spectrometer was realigned for more reliable sample spinning.
• The frequency synthesizer was modified by the NMR Facility Staff to include frequency markers.

External Funding and Pending Acquisitions
NSF and IU approved funding for a departmental solid-state NMR spectrometer. Negotiations with several spectrometer vendors is currently in progress. A 400 MHz widebore instrument will be purchased and installed by summer, 1999. Primary users will be the Caulton, Chisholm, and Zwanziger groups. The instrument will also be available to other members of the Department.

Continuing Projects

• The departmental solid-state NMR spectrometer will be purchased and installed by summer 1999.
• A 200 MHz superconducting magnet and spectrometer system will replace the T60 NMR spectrometer in the teaching laboratory by Spring 1999.
• All spectrometers and workstations will be made Y2000-compliant before the fall 1999 academic semester.
• Several new functionalities will be added to the MAG RES scheduling system.

1998 Graph Gallery
Data for the Graph Gallery was derived from NMR Facility accounting records from January 1 to December 31, 1998. These records were automatically generated from the spectrometer & datastation login/logout processes. All data is accurate to within 1 minute.

The Relative Utilization by Group pie charts show utilization by each group relative to total time used. The "Others" category of these pie charts represents the sum of groups that had less than 5% utilization of the spectrometer or datastations.

Back to NMR Facility Home Page
Send comments to: chemnmr@indiana.edu